US7910505B2 - Sintered glass ceramic and method for producing the same - Google Patents

Sintered glass ceramic and method for producing the same Download PDF

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US7910505B2
US7910505B2 US11/757,534 US75753407A US7910505B2 US 7910505 B2 US7910505 B2 US 7910505B2 US 75753407 A US75753407 A US 75753407A US 7910505 B2 US7910505 B2 US 7910505B2
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weight
glass
starting
except
sintering
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US20070281851A1 (en
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Karine Seneschal-Merz
Bernd Hoppe
Dirk Sprenger
Martin Letz
Thilo Zachau
Friedrich Siebers
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Schott AG
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Schott AG
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/062—Glass compositions containing silica with less than 40% silica by weight
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    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/062—Glass compositions containing silica with less than 40% silica by weight
    • C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
    • C03C3/068—Glass compositions containing silica with less than 40% silica by weight containing boron containing rare earths
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    • C03C4/00—Compositions for glass with special properties
    • C03C4/12—Compositions for glass with special properties for luminescent glass; for fluorescent glass
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    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/76—Crystal structural characteristics, e.g. symmetry
    • C04B2235/762—Cubic symmetry, e.g. beta-SiC
    • C04B2235/764—Garnet structure A3B2(CO4)3

Definitions

  • the present invention relates to a sintered glass ceramic, to a method for producing the same and to an advantageous application of such a sintered glass ceramic.
  • LEDs have been employed to an increasing degree for lighting purposes because they offer a number of advantageous properties including, for example, high efficiency due to direct conversion of electric energy to light energy, and high compactness.
  • LEDs produce light in a very narrow spectral band, while in most of the cases white light is required for illumination purposes.
  • Commercially available white LEDs use a III-V semiconductor emitter for stimulating a luminescent material that emits a secondary wavelength in a lower wavelength band (down conversion).
  • One known solution uses a blue InGaN/GaN LED for stimulating YAG:Ce, a broadband yellow luminescent material. With these LEDs, that have been converted using a luminescent material, a given proportion of the emitted blue light passes the luminescent layer covering the LED chip so that the overall spectrum obtained assumes a color very close to white light. Due to the absence of spectral portions in the blue/green band and in the red wavelength band, the resulting color is, however, not satisfactory in most of the cases.
  • US 2003/0025449 A1 discloses a hybrid LED comprising a radiation-emitting semiconductor body (chip) which is in direct contact, via an optical coupling agent, with a glass ceramic body that serves as a conversion agent.
  • the glass ceramic body contains crystallites of the garnet type doped with rare earths (such as YAG:CE), thiogalate or chlorosilicate as luminescent material.
  • the starting glasses from which such glass ceramics are produced consist of silicate glasses or borate glasses.
  • the luminescent glass ceramic is produced by mixing a glass frit with a suitable proportion of a luminescent material in powder form, and the mixture is molten, then cast and molded to achieve the desired shape. It is possible in this way, from the very beginning, to produce a glass ceramic body in the desired shape, advantageous for the intended application, for example in the form of a lens.
  • EP 1 642 869 A1 discloses a glass ceramic which preferably is used for down-conversion of excitation radiation in the blue and UV regions of the spectrum.
  • the glass ceramic comprises the following components (on an oxide basis): 5-50% by weight of SiO 2 , 5-50% by weight of Al 2 O 3 , 10-80% by weight of Y 2 O 3 , 0-20% by weight of B 2 O 3 0.1-30% by weight of rare earths, preferably 15-35% by weight of SiO 2 , 15-35% by weight of Al 2 O 3 , 25-60% by weight of Y 2 O 3 , 1-15% by weight of B 2 O 3 and 1-15% by weight of rare earths.
  • the glass ceramic contains crystalline phases in which rare-earth ions are taken up at least in part.
  • Crystalline phases containing yttrium ions as a component are replaced by rear-earth ions in this case at least in part.
  • the phases in question may include, for example, Y 3 Al 5 O 12 (YAG), Y 2 SiO 5 , Y 2 Si 2 O 7 , SrAl 2 O 4 , BaMgAl 10 O 17 , Sr 2 P 2 O 7 , Sr 4 Al 14 O 25 and YbO 3 , that serve as host phase for taking up rare-earth ions at least in part.
  • the respective glasses are produced by a technological melting process and may then be ceramized. Ceramization is effected by initial tempering at a nucleation temperature of between 850° C. and 900° C., for a period of several hours, and then ceramizing at a temperature of between 1050 to 1150° C. for the time of one hour.
  • the crystal phases identified in this case were Y 2 Si 2 O 7 , Y 2 SiO 5 , YbO 3 .
  • the conversion efficiency of such glass ceramics is, however, not yet sufficient for many applications because the glass ceramic contains a number of non-convertible crystal phases such as Y 2 Si 2 O 7 .
  • JP(A) H04-119941 further discloses a glass ceramic that contains 5-50% by weight of SiO 2 , 5-70% by weight of Al 2 O 3 , 10-70% by weight of Y 2 O 3 and 0.1 to 30% by weight of a nucleation agent such as MgO, TiO 2 , ZrO 2 or La 2 O 3 .
  • a nucleation agent such as MgO, TiO 2 , ZrO 2 or La 2 O 3 .
  • starting materials oxides
  • organic solvents and binders are heated to then form a shaped glass by solid-state reaction.
  • the glass so produced is then subjected first to a nucleation process, by tempering at temperatures of between 950° C. and 1010° C., and then to ceramization at a temperature of approximately 1100° C.
  • the production process is relatively complex. And in addition, the glass ceramic has a conversion efficiency not sufficient for all applications.
  • a glass ceramic product and a method for producing the same containing a garnet phase, a celsian crystal phase having the composition BaAl 2 Si 2 O 8 as well as at least one crystal phase having the composition AlN, Si 3 N 4 , SiC, Al 2 O 3 , ZrO 2 , 3Al 2 O 3 .2SiO 2 or Mg 2 SiO 4 .
  • Production is effected by sintering at a temperature of 700 to 1000° C.
  • the known glass ceramic is suited for use as an insulating substrate in a housing intended to accommodate semiconductor chips.
  • a glass ceramic known from U.S. Pat. No. 3,843,551 is used as luminescent laser material.
  • the glass ceramic consists of 45-68% by weight of SiO 2 , 15-30% by weight of Al 2 O 3 , 0-10% by weight of P 2 O 5 , 2-6% by weight of Li 2 O, 0-3% by weight of MgO, 0-8% by weight of ZnO, 2-7% by weight of ZrO 2 , 1-7% by weight of Ta 2 O 5 , 0-12 by % by weight of lanthanoids, as well as refining agents.
  • the glass ceramic is ceramized by tempering a starting glass over a plurality of hours at 800° C.
  • first object of the present invention to provide a method for producing a glass ceramic, whereby particularly advantageous radiation conversion properties can be achieved, in particular for down-conversion of LED radiation.
  • the invention is further realized by a sintered glass ceramic which is free from alkali oxides, except for incidental contamination, and which contains at least one garnet phase that contains at least one lanthanoid.
  • undesirable non-convertible crystal phases yttrium silicates, for example Y 2 Si 2 O 7 in different isotypes
  • the desired crystal phases doped with rare earths for example YAG (Y 3 Al 5 O 12 )
  • YAG Y 3 Al 5 O 12
  • the method according to the invention prevents such disadvantages found in the prior art by sintering a suitable starting glass until the desired garnet phase is formed. The formation of undesirable, non-convertible crystal phases is avoided in this way. The glass ceramic so produced provides very good conversion efficiency.
  • the glass ceramics according to the invention are produced by pressing fine powders (normally ⁇ 100 ⁇ m) of a starting glass in a mold and then simultaneously sintering and crystallizing that material by subsequent temperature treatment.
  • the resulting product contains considerable proportions of glassy products (glass ceramic >approximately 5% by vol. of glass phase, contrary to ceramics) and shows closed porosity of preferably ⁇ 10% by vol., more preferably ⁇ 5% by vol., most preferably ⁇ 1% by vol., depending on the starting particle size and the sintering conditions.
  • the starting glass used preferably is one that contains (on an oxide basis) 5-50% by weight of SiO 2 , 5-50% by weight of Al 2 O 3 and 10-80% by weight of a least one oxide selected from the group formed by Y 2 O 3 , Lu 2 O 3 , Sc 2 O 3 , Gd 2 O 3 , Yb 2 O 3 , Ce 2 O 3 , as well as 0.1-30% by weight of at least one oxide selected from the group formed by B 2 O 3 , Th 2 O 3 , and oxides of the lanthanoids, except Lu 2 O 3 , Gd 2 O 3 , Yb 2 O 3 , Ce 2 O 3 .
  • Such starting glasses are thermodynamically stable for being produced by a technical glass-production process (pot-melting or tank-melting).
  • an optimum with respect to particle size distribution, sintering temperature, heating rate and holding time at the sintering temperature is sought for the production of sintered glass ceramics in order to achieve maximum sintering and maximum crystallization of the desired phase and a minimum crystallite size for transparent/translucent glass ceramics.
  • Variants A, B and C are preferred embodiments of the invention. Combining the embodiments A, B and C is advantageous and preferred according to the invention.
  • inert glass to be added for variant C depends on the porosity that is to be expected considering the particle size distribution and the sintering conditions, which is to be closed by displacement.
  • porosity that is to be expected considering the particle size distribution and the sintering conditions, which is to be closed by displacement.
  • the sintering temperature of the starting glass Ts (G) is higher by at least 200 K than the processing temperature Va (I) of the inert glass,
  • the inert glass should have little tendency to crystallize at the sintering temperature (the upper devitrification limit of the inert glass OEG(I) serves as a measure in this respect), preferably: Ts(G) ⁇ OEG(I)>0 K more preferably: Ts(G) ⁇ OEG(I)>25 K.
  • the inert glass should permit high wetting of the starting glass G by the inert glass I. This is reached by chemical similarity between the glass I and the glass G: Both should be oxidic glasses.
  • the starting glass G should have chemical stability to attack by the molten inert glass I. There should be no inhibiting influence on the crystallization process of the starting glass G by the inert glass I (for example by diffusion processes).
  • the inert glass I acts as a catalyst for crystallization in the starting glass G.
  • the inert glass should have high optical transparency to excitation light and fluorescent light.
  • the inert glass should have a high index of refraction n d (I) at a low Abbe's coefficient V d (I), preferably adapted to the desired lanthanoid-doped crystal phase such as Ce:YAG.
  • the index of refraction of the inert glass I is advantageous according to the invention because, when the indices of refraction are well adapted, coupling-in the blue excitation light into the YAG crystals and coupling-out the yellow fluorescent light from the crystals are effected without substantial losses by total reflection and reflection at the YAGlinert glass phase boundaries. Low light losses due to optical aberration are achieved by the low Abbe's coefficient of the glass (I).
  • a first embodiment of a suitable inert glass comprises 0.5-1.5% by weight of SiO 2 , 28-34% by weight of B 2 O 3 , 0.1-0.3% by weight of BaO, 1.5-4% by weight of ZnO, 43-49% by weight of La 2 O 3 , 7-11% by weight of Y 2 O 3 , 2.5-4% by weight Nb 2 O 5 , 6-8% by weight of ZrO 2 and 0.3-1% by weight of WO 3 .
  • a second embodiment of a suitable inert glass comprises 4-6% by weight of SiO 2 , 19-23% by weight of B 2 O 3 , 21-27% by weight of ZnO, 34-40% by weight of La 2 O 3 , 6-8% by weight of Nb 2 O 5 , 3-5% by weight of ZrO 2 and 0.5-1.5 WO 3 .
  • a third embodiment of a suitable inert glass comprises 4-7% by weight of SiO 2 , 18-21% by weight of B 2 O 3 , 22-25% by weight of ZnO, 34-39% by weight of La 2 O 3 , 7-9% by weight of Nb 2 O 5 , 4-7% by weight of TiO 2 and 2-4% by weight of ZrO 2 .
  • Temperature treatment is preferably controlled so that during ceramization a crystal phase content of 10 to 95%, more preferably of 20 to 80%, most preferably of 25 to 75%, is obtained in a residual glass phase.
  • the at least one garnet phase is a phase of the type A 3 B 2 C 3 O 12 , wherein
  • location B can be taken by a trivalent lanthanoid cation such as Ce 3+ . Due to the small spacing to the next oxygen atoms, the tetrahedron locations can accommodate a small cation only, such as aluminum or silicon. The octahedron location must in any case be occupied by a trivalent cation.
  • the garnet phases doped with at least one lanthanoid, produced during the ceramization process may be garnet phases such as Y 3 Al 5 O 12 (YAG), Lu 3 Al 5 O 12 (LuAG), Gd 3 Al 5 O 12 (GdAG), Yb 3 Al 5 O 12 (YbAG), Y 3 Sc 2 Al 3 O 12 , Y 3 Sc 2 Al 3 O 12 , Lu 3 Sc 2 Al 3 O 12 , Gd 3 Sc 2 Al 3 O 12 and Yb 3 Sc 2 Al 3 O 12 .
  • they may be Ce 0.09 Y 2.91 Al 5 O 12 .
  • a garnet phase is produced during ceramization which is doped with at least one element selected from the group formed by the lanthanoids cerium, lanthanum, praseodymium, neodymium, samarium, europium, terbium, dysprosium, holmium, erbium, thulium and thorium.
  • a glass ceramic comprising a content of lanthanoids of 0.1 to 20% by weight, preferably 1 to 15% by weight, more preferably 2 to 10% by weight, is produced during ceramization.
  • the content of lanthanoids in the glass ceramic can be adapted in this way to the desired conversion task in order to achieve the best possible conversion result.
  • the starting glass used preferably is free from alkali oxides, further from PbO, further free from TiO 2 , further free from MgO, and preferably free from ZrO 2 .
  • the starting glass used preferably comprises the following components (in % by weight on an oxide basis):
  • the starting glass used comprises the following components (in % by weight on an oxide basis):
  • the starting glass as well as the inert glass do not contain any further components, apart from the components explicitly given and apart from refining agents and incidental contamination.
  • the term “incidental contamination” is understood to be a contamination by a maximum amount of 0.5 per cent by weight, or when very pure ingredients are used, by a maximum amount of 0.1 per cent by weight, or even by a maximum amount of 0.05 per cent by weight.
  • the content of Y 2 O 3 may be replaced in full or in part by Lu 2 O 3 , Sc 2 O 3 , Gd 2 O 3 and/or Yb 2 O 3 .
  • the starting glass is one that contains no further components, except for refining agents and incidental contamination.
  • the lanthanoids preferably may be at least one of the elements cerium or europium, although the other lanthanoids may be used as well and, in addition, small quantities of other lanthanoids may be additionally doped for optimizing color location, color temperature and the color reproduction index.
  • Heating up to sintering temperature may be effected preferably using infrared radiation by short-wave infrared radiant (SIR) heaters.
  • SIR short-wave infrared radiant
  • a SIR heating unit suited for that purpose has been known, for example, from EP 1 171 392 B1 which is fully incorporated by reference in this regard.
  • the wall and roof surfaces of such a heating unit consist of a highly IR-reflective material such as quarzal.
  • the sample to be sintered is preferably placed in this case on a support in powder form, consisting for example of Al 2 O 3 powder or SiO 2 powder.
  • the support used may alternatively also consist of quartz glass or another high-melting glass.
  • the support may consist of platinum or another highly IR-absorbing material.
  • a glass ceramic produced according to the invention preferably is used as radiation conversion body for converting a first radiation into a radiation with a different energy content or a different spectral distribution, preferably for down-conversion of excitation radiation in the blue and the UV region of the spectrum.
  • the radiation conversion body is produced in a thickness of 0.01 to 0.5 mm, preferably 0.05 to 0.2 mm.
  • the radiation conversion body is produced in a length of 0.1 to 10 mm, preferably 0.2 to 5 mm, more preferably 0.5 to 2 mm.
  • Such a geometry allows the body to be suitably adapted to the solid-state transitions of the respective LED chips.
  • FIG. 1 shows a scanning electron microscope pattern (SEM) of a glass ceramic produced according to the invention
  • FIG. 2 shows a detail of FIG. 1 that illustrates the different crystal phases.
  • the glass ceramics according to the invention are produced by pressing fine powders (particle size normally ⁇ 100 ⁇ m) of a starting glass in a mold and then simultaneously sintering and crystallizing the material by subsequent temperature treatment.
  • the product so obtained contains, in addition to crystalline phases, considerable portions of glassy materials (glass ceramics >approximately 5% by vol. of glass phase, in contrast to ceramics) and shows closed porosity, depending on the starting particle size and the sintering conditions.
  • Table 1 summarizes different compositions of starting glasses that are used for production of the glass ceramics according to the invention.
  • the starting glasses used all are thermodynamically stable, for being produced by a technical glass production process (pot-melting or tank-melting) and for being molded by a technical hot-molding process.
  • the starting glasses G1 to G9 (compare Table 1) are molten in platinum melting pots at a temperature of approximately 1550 to 1600° C. and are homogenized. After cooling down to room temperature, a homogeneous, clear, transparent glass is obtained. The glasses obtained are quenched and ground.
  • Table 3 contains under “Variant A” seven Examples Nos. 1 to 7 that have been sintered under vacuum in order to achieve the lowest possible porosity.
  • 100 g of the respective glass G7 of the stated particle size fraction (d50; d90) were isostatically cold-pressed at a pressure of 6300 bar, to a sample size of 1.5 ⁇ 1 ⁇ 3 cm.
  • the samples were placed in the pre-heated sintering furnace, were isothermally sintered for the stated sintering time, whereafter the furnace was switched off and the samples were removed after they had cooled down.
  • Example No. 3 Except for Example No. 3, all samples yielded transparent glass ceramics that predominantly contained a YAG phase.
  • the porosity for Examples Nos. 3 to 7 is smaller than 5 ⁇ m in all cases and, accordingly, is sufficiently low for most of the applications.
  • a bimodal particle size distribution of the starting powder of the sintered glass ceramics is obtained when differently fine powders of the starting glasses are intimately mixed in advantageous ratios before they are pressed and sintered.
  • Advantageous mixtures of such particle fractions are mixed in ratios that on the one hand increase the packing density while, on the other hand, they do not obstruct common sintering by surface crystallization effects that take place more rapidly in a smaller particle.
  • the factor depends on the width of the particle size distribution of powders 1 and 2 .
  • another variant suited for achieving very low porosity, consists in admixing a glass frit of an inert glass I to the glass frit of the starting glass, where the inert glass is already liquid at the sintering temperature Ts of the starting glass thereby filling the cavities between neighboring particles by viscous flowing.
  • compositions of possible inert glasses 11 to 15 are summarized in Table 2.
  • Example 9 An example of that kind, which has been produced using the inert glass 15, is listed as Example 9 in Table 3 under “Variant C” (otherwise identical pressing and sintering conditions as for Examples 1-8).
  • the pore size is below 1% by vol.
  • the crystal phase detected was predominantly YAG.
  • FIGS. 1 and 2 show a SEM pattern of a sample from Example No. G7 in Table 1. The pores are indicated by reference numeral 10 .
  • a crystallite 12 comprises a marginal YAG phase 14 and a core 16 of mullite.
  • Glass I4 for example, has an index of refraction of 1.8 at 588 nm and an Abbe's coefficient of 41.3.

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US20110062393A1 (en) 2011-03-17
DE102006027307B4 (de) 2014-08-07
FR2901784A1 (fr) 2007-12-07
DE102006027307A1 (de) 2007-12-13
FR2901784B1 (fr) 2010-11-12

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